Method for purification of vinyl polymers

Inactive Publication Date: 2002-09-19
KANEKA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the vinyl polymer produced by atom transfer radical polymerization contains residues of the transition metal complex used as the polymerization catalyst, so that troubles such as discoloration and adverse effects on physical properties of the product polymer as well as environmental safety problems are at times encountered.
Taking an alkenyl group-terminated vinyl polymer produced by utilizing said atom transfer radical polymerization technique as an example, the residual catalyst acts as a catalyst poison in hydrosilylation to interfere with the hydrosilylation reaction so that the expensive transition metal catalyst has to be used in a substantial amount.
However, this practice tends to require a large quantity of the adsorbent entailing an increased burden on the environment associated with the subsequent disposal of the adsorbent and an increased production cost.
If the molecular weight is too low, the inherent characteristics of vinyl polymers will not be fully expressed.
If, conversely, it is too high, the polymer will be hard to work with.
If the amount is less than 10-8 mol, the curing reaction will not proceed well.
Moreover, since hydrosilylation catalysts in general are expensive and corrosive, a substantial amount of hydrogen gas maybe evolved to cause foaming in the cured product.
At amounts below 0.01 parts by weight, the adhesion-improving effect will be insufficient.
On the other hand, if the amount of 20 parts by weight is exceeded, the physical properties of the cured product will be adversely affected.

Method used

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  • Method for purification of vinyl polymers
  • Method for purification of vinyl polymers
  • Method for purification of vinyl polymers

Examples

Experimental program
Comparison scheme
Effect test

production example 2

(Production Example 2)

[0295] A 50 L autoclave equipped with a reflux condenser and stirrer was charged with a suspension of CuBr (251.82 g, 1.76 mol) in acetonitrile (2640 g) and, after nitrogen sealing, the suspension was stirred at 65.degree. C. for 30 minutes. Then, butyl acrylate (6.0 kg), diethyl 2,5-dibromoadipate (526.70 g, 1.46 mol), acetonitrile (695 g) and pentamethyldiethylenetriamine (12.0 mL, 58.5 mmol) (hereinafter briefly as triamine) were added and the reaction was started. Under stirring at 80.degree. C., butyl acrylate (24.0 kg) was continuously added dropwise. In the course of dropwise addition of butyl acrylate, a further amount of triamine (36.0 mL, 176mmol) was added. Afterheating and stirring at 80.degree. C., 1,7-octadiene (6.448 kg) and triamine (120.0 mL, 585 mmol) were added and the mixture was further stirred under heating at 80 .degree. C for 4 hours. Thereafter, the heating and stirring were stopped for a while and a further amount of triamine (80.OmL, ...

example 1

(Example 1)

[0300] To 15 mL of polymer solution [1'] was added sodium percarbonate (1.00 g; product of Mitsubishi Gas Chemical; powders), and the mixture was stirred at room temperature for 3 hours. After the solid fraction was filteredoff, thetoluene was distilled off to give a vinyl polymer. Using the polymer thus obtained, the residual copper was determined. The result is shown in Table 1.

example 2

(Example 2)

[0302] To 40 mL of polymer solution [2'] was added sodium percarbonate (2.00 g; product of Mitsubishi Gas Chemical; powders), and the mixture was stirred at room temperature for 3 hours. The solid fraction was filtered off and the toluene was distilled off to give a vinyl polymer. Using the polymer thus obtained, gelation time and residual copper were determined. The results are shown in Table 1.

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Abstract

This invention provides a method for purification of a vinyl polymer which comprises the atom transfer radical polymerization of a vinyl monomer using a transition metal complex as the polymerization catalyst, said vinyl polymer being brought into contact with an oxidizing agent or a reducing agent.

Description

[0001] The present invention relates to a method for purification of vinyl polymers, vinyl polymers, hydrosilylatable compositions, and curable compositions.PRIOR ART[0002] The hydrosilylation reaction is used for functional group transformation or crosslinking, for instance, and as such is one of reactions of great industrial importance. By way of illustration, it is known that a polymer having an alkenyl functional group at its molecular chain terminus undergoes crosslinking in the presence of a hydrosilyl group-containing compound as a curing agent to give a cured product of good heat resistance and durability and that the reaction of such an alkenyl group-terminated polymer with a crosslinkable silyl group-containing hydrosilyl compound gives a crosslinkable silyl group-terminated polymer. While such a hydrosilylation reaction proceeds under heating, a hydrosilylation catalyst is generally added for accelerating the reaction. As examples of said hydrosilylation catalyst, radical...

Claims

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Application Information

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IPC IPC(8): C08F6/02C08F8/04C08F8/06C08F8/42
CPCC08F6/02C08F8/04C08F8/06C08F8/42
InventorFUJITA, NAOKITANO, KENICHINAKAGAWA, YOSHIKI
OwnerKANEKA CORP